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Preparation method for cefotetan disodium

A technology of cefotetan disodium and cefotetan acid, which is applied in the field of medicine, can solve problems such as poor clarity, dark product color, and solvent residue content, and achieve easy raw materials, low content, and polymer and related substance content low effect

Active Publication Date: 2014-12-10
CHINA MEHECO SANYANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In view of this, the technical problem to be solved in the present invention is to provide a kind of preparation method of cefotetan disodium, to solve the problem that when the traditional method produces cefotetan disodium, the color of the product is dark, the clarity is poor, solvent residue and related substance content high problem

Method used

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  • Preparation method for cefotetan disodium
  • Preparation method for cefotetan disodium
  • Preparation method for cefotetan disodium

Examples

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[0055] The present invention provides a method for preparing cefotetan disodium, and those skilled in the art can learn from the content of this article and appropriately improve the process parameters. In particular, it should be pointed out that all similar substitutions and modifications are obvious to those skilled in the art, and they are all deemed to be included in the present invention. The method and application of the present invention have been described through the preferred embodiments. It is obvious that relevant persons can modify or appropriately change and combine the methods and applications described herein without departing from the content, spirit and scope of the present invention to achieve and Apply the technology of the present invention.

[0056] The present invention provides a method for preparing cefotetan disodium. First, take cefotetan acid to form a first salt and mix it with silica gel, collect the first filtrate through the first filtration, and ...

Embodiment 1

[0080] Example 1 Preparation of Cefotetan Acid

[0081] 30.00kg of 7β-amino-7α-methoxy-3-[(1-methyl-1H-tetrazol-5-yl)thiomethyl]-3-cephem-4-carboxylic acid benzhydryl (7-MAC) was added to a 500L enamel reactor filled with 180L of dichloromethane, stirred for 30 minutes to dissolve, cooled to -20°C, added 10.5kg of N,N-dimethylaniline and 16.5kg of bromoacetyl bromide, After reacting for 1 hour, the reaction solution was washed with 30L ice water, 30L saturated potassium hydrogen sulfate solution, 30L saturated sodium bicarbonate solution (stirring for 30 minutes each time, standing for 30 minutes), and layered, the methylene chloride layer was washed with 2kg After drying with sodium sulfate for 60 minutes, the filtrate was dried under reduced pressure at 40°C, and the solvent was recovered to obtain 25.2kg of residual oil, which is 7β-bromoacetamido-7α-methoxy-3-(1-methyl-1H) -5-tetrazolyl)thiomethyl-3-cephem-4-carboxylic acid benzhydryl;

[0082] Take 25kg of 7β-bromoacetamido-...

Embodiment 2

[0084] Example 2 Preparation of Cefotetan Acid

[0085] 30.00kg of 7β-amino-7α-methoxy-3-[(1-methyl-1H-tetrazol-5-yl)thiomethyl]-3-cephem-4-carboxylic acid benzhydryl (7-MAC) was added to a 500L enamel reactor filled with 300L of dichloromethane, stirred for 60 minutes to dissolve, cooled to -30°C, added 13.5kg of N,N-dimethylaniline and 21.0kg of bromoacetyl bromide, After reacting for 1 hour, the reaction solution was washed with 60L ice water, 60L saturated potassium hydrogen sulfate solution, 60L saturated sodium bicarbonate solution in sequence (stirring for 30 minutes each time, standing for 30 minutes), layering, the dichloromethane layer with 4kg After drying with sodium sulfate for 60 minutes, the filtrate was dried under reduced pressure at 40°C, and the solvent was recovered to obtain 25.4 kg of residual oil, which is 7β-bromoacetamido-7α-methoxy-3-(1-methyl-1H) -5-tetrazolyl)thiomethyl-3-cephem-4-carboxylic acid benzhydryl;

[0086] Take 25kg of 7β-bromoacetamido-7α-m...

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Abstract

The invention relates to the technical field of medicine and particularly relates to a preparation method for cefotetan disodium. In the preparation method, cefotetan acid is mixed with silica gel through a first salifying, then a first filter liquor is collected through a first filtering, the first filter liquor is mixed with EDTA and active carbon, a second filter liquor is collected through filtering, then acid-forming and crystallization are performed, and then cefotetan acid product is obtained through third filtration, collection and filter cake, as well as washing; and the cefotetan acid product is taken to be mixed with active carbon after second salifying, fourth filter liquor is collected through the fourth filtering, and then degerming and freeze drying are performed, namely the cefotetan disodium is obtained. The product prepared by using the method provided by the invention is white, is excellent in solution clarity after solution, is less in the variety of residual solvent, is low in content of relevant matters such as polymer and the like, the adopted process is simple, the raw materials are easy to access, and the method is suitable for large-scale industrial production.

Description

Technical field [0001] The medical technology field of the present invention particularly relates to a preparation method of cefotetan disodium. Background technique [0002] Cefotetan disodium is an antibiotic with a structure as shown in Formula I. It was first developed by Fujisawa Corporation of Japan in 1979 and first marketed in Japan in the late 1980s. FDA approved as a new drug on December 27, 1985 (Cefotetan disodium sterile powder injection) was launched in the United States. [0003] [0004] Formula 1 [0005] Cefotetan is the drug with the longest half-life of the second-generation cephalosporins (cephalosporins) so far. Cefotetan and penicillin binding protein have a strong affinity and binding. It blocks the synthesis of bacterial cell wall mucopeptides, thereby exerting its antibacterial activity. Because the 7-position carbon atom on the β-lactam ring has a methoxy group, it is extremely stable to β-lactamases (including penicillinase and cephalosporinase) produc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/57C07D501/04C07D501/12
Inventor 张鹏飞秦坤贤刘玮朱峰李锦云
Owner CHINA MEHECO SANYANG PHARMA CO LTD
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